CN102031569B

CN102031569B - Method for producing silk glue-enriched silk spinning refined silk

Info

Publication number: CN102031569B
Application number: CN2010105454125A
Authority: CN
Inventors: 席星航; 李龙
Original assignee: 席星航
Current assignee: Hubei four new silk Medical Technology Co Ltd
Priority date: 2010-11-16
Filing date: 2010-11-16
Publication date: 2012-02-29
Anticipated expiration: 2030-11-16
Also published as: CN102031569A

Abstract

The invention relates to a method for producing silk glue-enriched silk spinning refined waste silk. In the method, the silk spinning refined waste silk retaining most of silk glue that is difficult to dissolve in a subsequent finishing process is obtained finally by softening, glue maintaining, oxidizing, cleaning and drying. Products prepared by the method have the characteristic that the cost is less than that of the conventional silk spinning refined waste silk and keep spongy and soft simultaneously, and the problem that the silk spinning refined waste silk produced by the conventional glue setting and softening technology yellows with heat is solved. Therefore, the silk spinning refined waste silk can adapt to the subsequent finishing process of silk spinning and blending and, after being carded simply, also can be used as fillers for producing waterproof mattresses or washable thermal appliances and the like, has wide application range and can create great economic benefit.

Description

Be rich in the production method of the silk spinning refined silk of silk gum

Technical field

The invention belongs to silk spinning industry, relating in particular to a kind of silk without the loose fiber shape that comes unstuck or do not come unstuck fully is raw material, processes the production method of the silk spinning refined silk that is rich in silk gum through protecting gum softening.

Background technology

The used refined silk of silk silk spinning industry mainly be utilize can not filature light defective cocoon and silk reeling process in the raw materials such as type of telling, recotti, husks that produce pass through refinery practice; Mainly be at first white silk through rare soap solution; Multiple practice etc. process will contain 10%--45% silk gum remove (because of silk gum water-soluble), to obtain removing refined silk most silk gum, fibrous, soft.Its utilization rate of raw materials of product that this method obtains is low, and the silk gum waste water of sloughing is also wanted contaminated environment.Therefore, in refining, keep silk gum as far as possible, change the water-soluble characteristic of silk gum, improving stock utilization is a kind of direction of industry development.Chinese patent 200410022061.4 discloses about 2%～5% blaze silk that the outer sleave of a kind of silk cocoon partly accounts for silk cocoon is processed the silk spinning refined silk that is rich in silk gum through fixed gum softening preparation method; Solved the problem of using behind the solid glue of blaze silk preferably; But owing to adopt glutaraldehyde as crosslinking agent; Therefore no matter how silk fiber drifts, be prone to flavescence once meeting the heating silk fiber, greatly limitations its actual application value.

Summary of the invention

The purpose of this invention is to provide a kind of production method that is rich in the silk spinning refined silk of silk gum, the mulberry silk refined silk that adopts this method to make to produce not only is rich in silk gum, and heats not flavescence, and is soft.

The method of the invention is carried out as follows:

A, softening process: a kind of silk without the loose fiber shape that comes unstuck or do not come unstuck is fully put into more than or equal to the mass ratio of 1:12 by solution in the solution of pH value 2～10 and flooded 20～120 minutes.

Above-mentioned being meant without the silk raw material that comes unstuck passed through the material of machine with fiber opening.The silk raw material that does not come unstuck fully is meant the used leftover bits and pieces of silk spinning after rare soap solution is just practiced, and silk gum is not practiced the loose material of fiber of falling fully, like machine silk floss, bar type of telling etc.

B, protect the glue process: will softening silk after the processing, to put into pH be that 3～10 tetra methylol phosphonium salt solution soaked 0.5～20 hour, and this tetra methylol phosphonium salt solution concentration is 0.03%～10%, and soaking temperature is 10 ℃～60 ℃; Bath raio is more than or equal to 1:10.

The present invention selects for use tetra methylol phosphonium salt solution to make crosslinking agent, can make the abundant set of silk gum, and is no longer water-soluble, heats not flavescence.

This step also can adopt the silk raw material after will soaking from tetra methylol phosphonium salt solution, to take out promptly 8～40 hours cold rolling heap a period of time, and the constant guarantor's glue of other process conditions is handled.

C, oxidizing process: will pass through that the silk of protecting gum softening is put into sodium perborate or hydrogen peroxide solution soaked 1～24 hour, the concentration of this solution is 0.2%～4%.This oxidizing process is carried out at normal temperatures.Bath raio is more than or equal to 1:15.

D, cleaning, drying process: the silk after the oxidation is cleaned, dewaters, obtain being rich in the silk gum silk spinning refined silk of (promptly having kept most of silk gum) being lower than to dry under 150 ℃ the temperature.

In above-mentioned steps, the purpose of softening process is to make the silk gum swelling; The purpose of protecting the glue process is to let soup and silk gum fully react, and changes that silk gum is prone to dissolve and the character of weak acid resistant weak base not; The purpose of oxidizing process is to let the abundant set of the inadequate silk gum of a small amount of set or come off, and makes the whole set quality of silk gum uniform and stable.

The present invention and Chinese patent 200410022061.4 disclosed blaze silk fixed gum softenings are processed the method for silk spinning refined silk relatively like following table:

The advantage that the present invention has is: the product cost that makes is low, and the pine bubble is soft, meets not flavescence of heat.The silk spinning refined silk of processing like this can adapt to the postorder arranging process of silk spinning, blending, and simply combing is not feared warming article that the mattress of water maybe can wash etc. as filler production yet, is with a wide range of applications and economic benefit greatly.

The specific embodiment

Embodiment one:

It is continuous without the machine of the loose fiber shape that comes unstuck to take by weighing 1000g, puts in the sodium hydroxide solution of 12 kilograms of pH=9 softeningly, takes out dehydration after 1 hour; Put into 12 kilogram of 5% tetra methylol sulfuric acid phosphorus solution again and protect glue, the pH=5 of tetra methylol phosphonium salt solution, soaking temperature are 40 ℃; After treating 5 hours; With the silk solution oxidation that to put into 15 kilograms of concentration be 0.5% sodium perborate, soak at normal temperatures after 5 hours and take out, dehydration, clean, oven dry; Bake out temperature is 120 ℃, obtains being rich in the silk spinning refined silk 1000g of silk gum.

Embodiment two:

The bar that takes by weighing the loose fiber shape that 500g do not come unstuck is fully told, and puts in the sodium carbonate liquor of 10 kilograms of pH=7 softeningly, takes out dehydration after 3 hours; Putting into 10 kilogram of 3% tetra methylol sulfuric acid phosphorus solution again soaks; The pH=3 of tetra methylol phosphonium salt solution, soaking temperature is 20 ℃, treats after 10 hours bar told that to put into 20 kilograms of concentration be 3% hydrogen peroxide solution oxidation; Soak at normal temperatures after 20 hours and take out; Dewater, clean, put into the dryer oven dry, bake out temperature is 80 ℃, obtains being rich in the silk spinning refined silk 500g of silk gum.

Embodiment three:

Take by weighing the husks of the loose fiber shape that 1000g do not come unstuck fully, put in the sulfuric acid solution of 20 kilograms of pH=3.5 softening; Treat to take out dehydration after 0.5 hour, put into 10 kilogram of 8% tetra methylol sulfuric acid phosphorus solution again and protect glue, the pH=5 of tetra methylol phosphonium salt solution; Soaking temperature is 40 ℃, treat 8 hours after, put into 4% hydrogen peroxide solution oxidation again; Soak at normal temperatures after 10 hours and take out; Dewater, clean, dry, bake out temperature is 100 ℃, promptly obtains being rich in the silk spinning refined silk 1000g of silk gum.

Claims

1. production method that is rich in the silk spinning refined silk of silk gum is characterized in that making as follows:

A, softening process: a kind of silk without the loose fiber shape that comes unstuck or do not come unstuck is fully put into more than or equal to the mass ratio of 1:12 by solution in the solution of pH value 2～10 and flooded 10～120 minutes;

B, protect the glue process: will softening silk after the processing, to put into pH be that 3～10 tetra methylol phosphonium salt solution soaked 0.5～20 hour, and this tetra methylol phosphonium salt solution concentration is 0.01%～10%, and soaking temperature is 10 ℃～60 ℃, and bath raio is more than or equal to 1:10;

C, oxidizing process: will pass through that the silk of protecting gum softening is put into sodium perborate or hydrogen peroxide solution soaked 1～24 hour, the concentration of this solution is 0.2%～4%; Bath raio is more than or equal to 1:15;

D, cleaning, drying process: the silk after the oxidation is cleaned, dewaters, dry the silk spinning refined silk that obtains being rich in silk gum being lower than under 120 ℃ the temperature.

2. according to the said production method that is rich in the silk spinning refined silk of silk gum of claim 1, it is characterized in that: said tetra methylol phosphonium salt is tetra methylol sulfuric acid phosphorus or THPC.